2025-04-072025-04-072025Hernández Salvador, S., Márquez Escudero, I., Gutiérrez Tarriño, S., Calvente Pacheco, J.J., Río Rodríguez, J.L.d., Oña Burgos, P.,...,Olloqui Sariego, J.L. (2025). Selective Design of MOF-derived Electrocatalytic Interphases by Potential-driven Surface Reconstruction. Electrochimica Acta, 525, 146158. https://doi.org/10.1016/j.electacta.2025.146158.1873-38590013-4686https://hdl.handle.net/11441/171535Metal-organic frameworks (MOFs) can be used as precursors for the directed synthesis of derived materials with enhanced performance for electrocatalysis. Herein, we report on an in-situ electrochemical strategy for the selective synthesis of hybrid electrocatalysts using a cobalt MOF (2D-CoMOF) as a precursor for constructing electrochemical sensors to monitor the glucose oxidation reaction (GOR). By using in-situ Raman spectroelectrochemistry, it is demonstrated that a precise control of the applied potential during amperometric treatment of 2D-CoMOF can promote the generation of derived heterostructures in which the original MOF coexists with metal oxides and/or oxyhydroxides (MOF-MOx) with different compositions. The so-prepared electrodes exhibit high electroactive surface areas, a high number of electrocatalytically active cobalt sites and an efficient charge transport across the catalytic film. Moreover, their composition-dependent electrocatalytic performance for the glucose oxidation reaction is examined, establishing a relationship between the applied potential, the macroscopic chemical composition of the heterostructure and the electrocatalytic performance for glucose sensing. In particular, the hybrid phases consisting of Co-MOF/Co3O4/CoOOH display superior electrocatalytic sensing performance with a wide linear concentration range and high sensitivity. The present work emphasizes the significance that the precise control of the applied potential has on the electrochemically-assisted MOF transformation for developing highly efficient MOF-derived electrocatalysts.application/pdf11 p.engAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/MOF-derived electrocatalystMOF surface reconstructionOperando raman spectroelectrochemistryGlucose oxidation reactioninfo:eu-repo/semantics/articleinfo:eu-repo/semantics/embargoedAccess10.1016/j.electacta.2025.146158